CN103730619B - 一种高强度的锂离子电池用隔膜的制备方法 - Google Patents

一种高强度的锂离子电池用隔膜的制备方法 Download PDF

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CN103730619B
CN103730619B CN201310604027.7A CN201310604027A CN103730619B CN 103730619 B CN103730619 B CN 103730619B CN 201310604027 A CN201310604027 A CN 201310604027A CN 103730619 B CN103730619 B CN 103730619B
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袁宏亮
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Abstract

本发明提供了一种锂离子电池用隔膜的制备方法，属于电池制造技术领域。包括如下步骤：第1步、取聚乙烯、二氧化钛、聚丙烯酰胺、聚丁二烯二醇、二羟甲基丙酸、过氧化二苯甲酰、聚环内酯、增塑剂，混合均匀，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；取氧化锆、纤维素、白炭黑、分散剂、溶剂，混合均匀，得到混悬液；第3步、将基材薄膜加热，然后在该温度下，将混悬液涂于基材薄膜上，升温，放冷，即可。本发明通过基材与涂层两部分的良好结合来实现隔膜的优异性能，首先，制备得到的基材薄膜具有良好的机械与绝缘性能，再通过加热互熔的方式，使涂层与基材之间协同作用，进一步地提高了隔膜的机械性能。

Description

一种高强度的锂离子电池用隔膜的制备方法
技术领域
本发明提供了一种锂离子电池用隔膜的制备方法，特别是涉及一种具有较高拉伸强度的隔膜的制备方法，属于电池制造技术领域。
背景技术
锂离子电池是一种充电电池，它主要依靠锂离子在正极和负极之间移动来工作。当对电池进行充电时，电池的正极上有锂离子生成，生成的锂离子经过电解液运动到负极。而作为负极的碳呈层状结构，它有很多微孔，达到负极的锂离子就嵌入到碳层的微孔中，嵌入的锂离子越多，充电容量越高。同样，当对电池进行放电时(即我们使用电池的过程)，嵌在负极碳层中的锂离子脱出，又运动回正极。回正极的锂离子越多，放电容量越高。
在锂离子电池中，隔膜的作用主要有两个方面：一方面起到分隔正、负极，防止短路的作用；另一方面，隔膜能够让锂离子通过，形成充放电回路。隔膜性能的优劣直接影响着电池内阻、放电容量、循环使用寿命以及安全性能。隔膜越薄，孔隙率越高，电池内阻越小，高倍率放电性能越好，性能优异的隔膜对提高电池的综合性能具有重要的作用。
锂离子电池对隔膜的要求。1.具有电子绝缘性，保证正负极的机械隔离；2.有一定的孔径和孔隙率，保证低的电阻和高的离子电导率，对锂离子有很好的透过性；3.耐电解液腐蚀，电化学稳定性好；4.对电解液的浸润性好并具有足够的吸液保湿能力；4.具有足够的力学性能，包括穿刺强度、拉伸强度等；5.空间稳定性和平整性好；6.热稳定性和自动关断保护性能好。
锂离子电池对隔膜采用的基体材料是聚烯烃材料，其具有优异的力学性能、化学稳定性和相对廉价的特点。隔膜基体材料主要包括聚丙烯、聚乙烯材料和添加剂。隔膜所采用基体材料对隔膜力学性能以及与电解液的浸润度有直接的联系。尽管近年来有研究用聚偏氟乙烯、纤维素复合膜等材料制备锂离子电池隔膜，但至今商品化的电池隔膜材料仍主要采用聚乙烯、聚丙烯微孔膜。
在锂离子电池隔膜的制造中，不仅要保持聚烯烃材料具有足够的机械强度，同时还要保证其的电学性能，具有较大的加工难度。
发明内容
本发明的目的是：提供一种具有较高机械强度的锂离子电池用隔膜，技术方案是：
一种高强度的锂离子电池用隔膜的制备方法，包括如下步骤：
第1步、按重量份计，取聚乙烯60～80份、二氧化钛5～10份、聚丙烯酰胺4～8份、聚丁二烯二醇1～3份、二羟甲基丙酸4～6份、过氧化二苯甲酰2～4份、聚环内酯1～3份、增塑剂2～4份，混合均匀，放入双螺杆挤出机的侧喂料斗，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；
第2步、按重量份计，取氧化锆15～20份、纤维素2～7份、白炭黑15～20份、分散剂2～4份、溶剂40～60份，混合均匀，得到混悬液；
第3步、将基材薄膜加热至90～110℃，保持15～30min，然后在该温度下，将混悬液涂于基材薄膜上，涂层厚度是2～4μm；升温至120～140℃，保持30～60min，放冷，即可。
优选地，第1步中，双螺杆挤出机的螺杆温度控制在190～210℃之间，螺杆的转速控制在140～160转/分钟。
优选地，所述的增塑剂是聚乙烯醇或者矿物油。
优选地，所述的纤维素是羟丙基甲基纤维素或者羟乙基纤维素中的一种。
优选地，所述的溶剂是N,N-二甲基丙烯酰胺。
有益效果
本发明通过基材与涂层两部分的良好结合来实现隔膜的优异性能，首先，制备得到的基材薄膜具有良好的机械与绝缘性能，再通过加热互熔的方式，使涂层与基材之间协同作用，进一步地提高了隔膜的机械性能，同时保持了良好的绝缘性能。
具体实施方式
实施例1
第1步、按重量份计，取聚乙烯60份、二氧化钛5份、聚丙烯酰胺4份、聚丁二烯二醇1份、二羟甲基丙酸4份、过氧化二苯甲酰2份、聚环内酯1份、增塑剂2份，混合均匀，放入双螺杆挤出机的侧喂料斗，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；
第2步、按重量份计，取氧化锆15份、纤维素2份、白炭黑15份、分散剂2份、溶剂40份，混合均匀，得到混悬液；
第3步、将基材薄膜加热至90℃，保持15min，然后在该温度下，将混悬液涂于基材薄膜上，涂层厚度是2μm；升温至120℃，保持30min，放冷，即可。
第1步中，双螺杆挤出机的螺杆温度190℃之间，螺杆的转速控制在140转/分钟。所述的增塑剂是聚乙烯醇，所述的纤维素是羟丙基甲基纤维素，所述的溶剂是N,N-二甲基丙烯酰胺。
实施例2
第1步、按重量份计，取聚乙烯80份、二氧化钛10份、聚丙烯酰胺8份、聚丁二烯二醇3份、二羟甲基丙酸6份、过氧化二苯甲酰4份、聚环内酯3份、增塑剂4份，混合均匀，放入双螺杆挤出机的侧喂料斗，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；
第2步、按重量份计，取氧化锆20份、纤维素7份、白炭黑20份、分散剂4份、溶剂60份，混合均匀，得到混悬液；
第3步、将基材薄膜加热至110℃，保持30min，然后在该温度下，将混悬液涂于基材薄膜上，涂层厚度是4μm；升温至140℃，保持60min，放冷，即可。
第1步中，双螺杆挤出机的螺杆温度210℃之间，螺杆的转速160转/分钟。所述的增塑剂是聚乙烯醇，所述的纤维素是羟丙基甲基纤维素，所述的溶剂是N,N-二甲基丙烯酰胺。
实施例3
第1步、按重量份计，取聚乙烯70份、二氧化钛7份、聚丙烯酰胺6份、聚丁二烯二醇2份、二羟甲基丙酸5份、过氧化二苯甲酰3份、聚环内酯2份、增塑剂3份，混合均匀，放入双螺杆挤出机的侧喂料斗，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；
第2步、按重量份计，取氧化锆17份、纤维素5份、白炭黑17份、分散剂3份、溶剂50份，混合均匀，得到混悬液；
第3步、将基材薄膜加热至100℃，保持20min，然后在该温度下，将混悬液涂于基材薄膜上，涂层厚度是3μm；升温至130℃，保持40min，放冷，即可。
第1步中，双螺杆挤出机的螺杆温度控制在200℃，螺杆的转速控制在150转/分钟。所述的增塑剂是聚乙烯醇，所述的纤维素是羟丙基甲基纤维素，所述的溶剂是N,N-二甲基丙烯酰胺。
性能试验
对实施例1～实施例3所得的锂离子电池用隔膜进行性能表征，并以专利CN1819306中的锂离子电池作对照。结果如下表所示。
实施例1 实施例2 实施例3 对照例
孔隙率％ 60％ 55％ 65％ 54％
孔径nm 50 55 45 80
纵向拉伸强度MPa 220 200 230 180
横向拉伸强度MPa 140 120 150 110
离子导电率σ/S·cm-1 3.3×10-3 3.4×10-3 3.1×10-3 5.6×10-3

Claims (1)

1.一种高强度的锂离子电池用隔膜的制备方法，其特征在于，包括如下步骤：
第1步、按重量份计，取聚乙烯70份、二氧化钛7份、聚丙烯酰胺6份、聚丁二烯二醇2份、二羟甲基丙酸5份、过氧化二苯甲酰3份、聚环内酯2份、增塑剂3份，混合均匀，放入双螺杆挤出机的侧喂料斗，进行熔融、混炼、挤出、冷却、干燥、切粒、制膜，得到基材薄膜；
第2步、按重量份计，取氧化锆17份、纤维素5份、白炭黑17份、分散剂3份、溶剂50份，混合均匀，得到混悬液；
第3步、将基材薄膜加热至100℃，保持20min，然后在该温度下，将混悬液涂于基材薄膜上，涂层厚度是3μm；升温至130℃，保持40min，放冷，即可；
第1步中，双螺杆挤出机的螺杆温度控制在200℃，螺杆的转速控制在150转/分钟；所述的增塑剂是聚乙烯醇，所述的纤维素是羟丙基甲基纤维素，所述的溶剂是N,N-二甲基丙烯酰胺。
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